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Thionyl Chloride → 4-Benzoyloxy-3-(2-pyridylazo)-1-naphthalenesulfonyl chloride

HRID 1395622
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HRID 1395622 반응식
[C:1]([O:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:13]([S:20](O)(=[O:22])=[O:21])=[CH:12][C:11]=1[N:24]=[N:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][N:27]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:34])=O>CN(C)C=O>[C:1]([O:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:13]([S:20]([Cl:34])(=[O:22])=[O:21])=[CH:12][C:11]=1[N:24]=[N:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][N:27]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 234561594-Benzoyloxy-3-(2-pyridylazo)-1-naphthalenesulfonic acid

생성물 1

HCID 234561604-Benzoyloxy-3-(2-pyridylazo)-1-naphthalenesulfonyl chloride

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-Benzoyloxy-3-(2-pyridylazo)-1-naphthalenesulfonic acid (70 g) was added to thionyl chloride (300 ml). Dimethylformamide (30 ml) was added in portions while the reaction mixture was being stirred. After 1 hour the starting material was all in solution. The reaction mixture was poured into a large quantity of ice after a further 4 hours' stirring. The product was filtered off and dissolved in chloroform. The chloroform layer was shaken with water to destroy any remaining thionyl chloride and dried over magnesium sulfate.

후처리

  1. additionThe reaction mixture was poured into a large quantity of ice after a further 4 hours'
  2. stirringstirring
  3. filtrationThe product was filtered off
  4. dissolutiondissolved in chloroform
  5. stirringThe chloroform layer was shaken with water
  6. customto destroy any remaining thionyl chloride
  7. dry with materialdried over magnesium sulfate

출처 및 근거

ORD 기록
ord-ee5e0f358a6d4f01adfc08be1239e31d
출처 데이터셋
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04204870

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